应用化学 ›› 2011, Vol. 28 ›› Issue (05): 608-610.DOI: 10.3724/SP.J.1095.2011.00434

• 研究简报 • 上一篇    

高岭土负载SO42-/ZrO2-TiO2催化剂的制备及其在缩酮合成中的应用

张恒*,王敏,朱万诚,李言信,赵斌   

  1. (曲阜师范大学化学与化工学院 曲阜 273165)
  • 收稿日期:2010-07-29 修回日期:2010-09-04 出版日期:2011-05-10 发布日期:2011-05-10
  • 通讯作者: 张恒,副教授; Tel:0537-4456301; Fax:0537-4456305; E-mail:ttlme@126.com; 研究方向:功能陶瓷与催化材料
  • 基金资助:
    山东省自然科学基金(Z2008B12)曲阜师范大学博士科研启动基金资助项目

Preparation of Kaolinite Supported SO42-/ZrO2-TiO2 Catalyst and Its Application in Cyclohexanon Ethylene Ketal Synthesis

ZHANG Heng*, WANG Min, ZHU Wancheng, LI Yanxin, ZHAO Bin   

  1. (School of Chemistry and Chemical Engineering,Qufu Normal University,Qufu 273165)
  • Received:2010-07-29 Revised:2010-09-04 Published:2011-05-10 Online:2011-05-10

摘要:

以经H2SO4处理焙烧的高岭土为载体,制备了以其负载的SO2-4/ZrO2-TiO2固体酸催化剂。 用FT-IR、XRD和NH3-TPD等测试技术表征了催化剂的微观结构及酸强度,考察了对环己酮乙二醇缩酮反应的催化活性及稳定性。 结果表明,酸化处理使高岭土表面酸量增加,但酸强度变化不大,而其负载SO2-4/ZrO2-TiO2后,经500 ℃焙烧3 h其酸量及酸强度显著升高。 环己酮用量为0.2 mol、乙二醇0.24 mol、催化剂1.2 g、带水剂环己烷15 mL,回流反应70 min后,缩酮收率可达96.8%,催化剂重复使用5次收率保持在90%以上。

关键词: 高岭土负载固体酸, 催化剂, 缩酮反应

Abstract:

Acid activated and kaolinite supported SO2-4/ZrO2-TiO2 was prepared as a solid acid catalyst. The structure and acid strength of the catalyst was studied by FT-IR, XRD and NH3-TPD. The activity and stability of the catalyst for the synthesis of cyclohexanon ethylene ketal were investigated. The results showed that the acid amount of kaolinite was increased with increasing acid activation, and the acid strength was significantly enhanced after supporting SO2-4/ZrO2-TiO2 and calcinations at 500 ℃ for 3 h. When the molar ratio of cyclohexanone to ethylene is 1∶1.2, the loading of catalyst is 1.2 g and the volume of cyclohexane is 15 mL, the yield of cyclohexanone ethylene ketal from 0.2 mol cyclohexanon feed could reach 96.8% after 70 min reaction. The catalyst was used repeatedly for 5 times with the yield still larger than 90%.

Key words: kaolinite supported solid acid, catalyst, ketalation

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